CN111690175A - Preparation method and application of rare earth composite antibacterial agent doped with nano silver - Google Patents
Preparation method and application of rare earth composite antibacterial agent doped with nano silver Download PDFInfo
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Abstract
The invention relates to a preparation method and application of a rare earth composite antibacterial agent doped with nano silver. The method comprises the steps of firstly preparing active carbon loaded nano zero-valent iron, namely, loading zero-valent iron powder on active carbon by using a dendrobe extracting solution; then, when preparing nano silver particles, doping nano silver on soluble rare earth salt to obtain modified rare earth salt; and finally, mixing the optimized components according to a ratio and calcining to obtain the three-phase antibacterial agent with stable performance. The whole method is simple and feasible, and the obtained antibacterial agent has lasting antibacterial effect, wide antibacterial spectrum and high environmental friendliness and is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of antibacterial agents, and particularly relates to a preparation method and application of a nano-silver doped rare earth composite antibacterial agent.
Background
The antibacterial agents are of various types and can be divided into the following components: biological antibacterial agents, inorganic antibacterial agents and organic antibacterial agents. Among them, the research and development of inorganic antibacterial agents have been remarkably advanced, and among them, novel antibacterial agents represented by rare earth complexes have been developed. Rare earths are popular in various fields because of their low toxicity, low side effects and broad-spectrum antibacterial activity. The principle of rare earth antibiotics is not explained in a unified manner. But a general consensus is that the bacteriostatic mechanism proposed by a. chaudhary: namely, the metal ions can act with cell walls, cell membranes, enzymes, proteins, DNA and RNA, and have stronger complexation with O, S, N atoms in the structures, thus interfering the normal physiological and biochemical functions of the bacteria, and further inhibiting the growth of the bacteria and even leading the bacteria to die. How to obtain a rare earth bacteriostatic agent with long bacteriostatic time and obvious antibacterial effect is a topic worthy of research.
CN106589582A discloses a reinforced and toughened antibacterial polypropylene material and a production method thereof, wherein nano zinc oxide or titanium dioxide is used as an inorganic antibacterial agent, then polypropylene, ultra-high molecular weight polyethylene master batches, the inorganic antibacterial agent, grafted polypropylene and other auxiliary agents are melted, blended and extruded by a double-screw extruder to obtain the reinforced and toughened antibacterial polypropylene material, however, when the method is applied to ultra-high molecular weight polyethylene (UHMWPE) fiber production, the antibacterial rate is greatly reduced, negative effects are generated on the breaking strength and the initial modulus, and in addition, TiO has negative effects on the breaking strength and the initial modulus2The inorganic antibacterial agent has antibacterial effect only under the condition of being excited by ultraviolet light, and has no antibacterial ability under other conditions, so the inorganic antibacterial agent has no universality and very limited application field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of a rare earth composite antibacterial agent doped with nano silver.
A preparation method of a rare earth composite antibacterial agent doped with nano silver comprises the following steps:
step 1, firstly preparing the loaded active carbon nano zero-valent iron
Firstly, taking activated carbon, cleaning, immersing the activated carbon into a dendrobium extract at a low temperatureTaking out after soaking for 24 hours, and carrying out vacuum drying for later use; secondly, taking 5-10g of treated active carbon and 100ml of 0.05mol/L FeSO4·7H2The O solution is reacted by adopting a liquid phase reduction method until no bubbles are generated, and the reaction is finished; thirdly, centrifugally separating a reaction product, ultrasonically cleaning for 3-5 times at 35 ℃, and drying in vacuum to obtain the loaded activated carbon nano zero-valent iron;
step 2, dissolving saturated fatty acid in a methanol water solution, adding sodium hydroxide into the solution to wash out a precipitate, filtering, and adding the precipitate into a silver nitrate solution to obtain saturated fatty acid silver; weighing saturated fatty acid silver, adding hexadecyl tertiary amine, electromagnetically stirring for 2 hours at the temperature of 60-70 ℃, then adding soluble rare earth salt, continuously stirring uniformly, precipitating, filtering, and drying in vacuum to obtain the modified rare earth salt, wherein the molar ratio of the soluble rare earth salt to the nano-silver is 1: 0.05-0.1;
weighing 25-38 parts of loaded activated carbon nano zero-valent iron, 8-14 parts of modified rare earth salt, 12-18 parts of potassium nitrate, 2-8 parts of sodium citrate, 8-14 parts of calcium stearate, 12-18 parts of sodium nitrate, 2-9 parts of potassium nitrate, 0.1-0.6 part of dispersant and 1-5 parts of lubricant by weight, mixing, grinding in a ball mill, calcining in a muffle furnace at 300 ℃ for 1-3 hours, and naturally cooling to obtain a semi-finished product;
and 4, repeatedly washing the semi-finished product, and drying in an oven to obtain the composite antibacterial agent.
As an improvement, the preparation of the dendrobium extract in the step 1 comprises the following steps: cutting stem of herba Dendrobii into segments with length of 1-2cm, adding 6-8 times of stem weight of herba Dendrobii into stem, extracting in water bath for 3-4 hr, and vacuum concentrating to obtain extractive solution.
As a modification, the eccentricity in step 1 was 4000-6000 rpm.
The improvement is that the soluble rare earth salt in the step 2 is cerium acetate, europium nitrate, lanthanum acetate or neodymium nitrate; the number of C in the saturated fatty acid is 10-14.
The improvement is that the components weighed in the step 3 are as follows: 30 parts of loaded activated carbon nano zero-valent iron, 12 parts of modified rare earth salt, 14 parts of potassium nitrate, 5 parts of sodium citrate, 10 parts of calcium stearate, 15 parts of sodium nitrate, 6 parts of potassium nitrate, 0.4 part of dispersant and 1 part of lubricant.
The improvement is that the temperature rise speed of the calcination in the step 3 is 5-10 ℃/min.
As an improvement, the specific steps of washing and drying in the step 4 are as follows: washing with ethanol and deionized water sequentially, circularly washing for 3-5 times, and drying in oven at 80 deg.C.
An antibacterial synthetic resin contains any one of the above rare earth complex antibacterial agent doped with nano-silver.
As an improvement, the bacteriostatic agent accounts for 0.01 to 0.5 percent of the mass of the bacteriostatic synthetic resin.
Has the advantages that:
compared with the prior art, the nano-silver doped rare earth composite antibacterial agent is prepared by optimizing and mixing the components of the antibacterial agent according to the proportion, the whole set of method is simple and easy to implement, the obtained antibacterial agent has lasting antibacterial effect and wide antibacterial spectrum, and is suitable for the antibacterial of synthetic resins, and the specific advantages are as follows:
1. the active carbon loaded nano zero-valent iron is used, the polysaccharide viscosity of the plant extract is adopted to effectively grid iron ions on the active carbon, the stability of the active carbon loaded nano zero-valent iron is ensured, the addition of organic adhesives is reduced, the environment friendliness is improved, in addition, the dendrobium extract has the antibacterial and bacteriostatic effects, and the antibacterial effect of the composite antibacterial agent is further improved;
2. the modified rare earth salt is prepared by adding the rare earth salt in the process of preparing nano silver to obtain a new layered metal dopant, and then mixing the new layered metal dopant with the loaded activated carbon nano zero-valent iron, so that the layered structure and the loaded structure can more easily form an embedded structure, common components of microorganisms can be more easily destroyed or dysfunction can be more easily generated, and ions penetrate through cell walls to enter cells and react with SH groups, so that protein is solidified, the sterilization effect is improved, and the bacteriostasis time is prolonged;
3. according to the invention, the dendrobium extract with natural bactericidal effect and various metals with antibacterial effect are mixed into a whole by a specific method, so that the use of organic matters is reduced in the preparation process, the environment friendliness is improved, the cost is reduced, the addition of antibacterial agent is reduced in the application process, the synthesis of functional resin is reduced, the cost is further reduced, and the dendrobium extract is suitable for industrialization.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
A preparation method of a rare earth composite antibacterial agent doped with nano silver comprises the following steps:
step 1, firstly preparing the loaded active carbon nano zero-valent iron
Firstly, cleaning activated carbon, soaking the cleaned activated carbon in a dendrobe extracting solution for 24 hours at low temperature, taking out the dendrobe extracting solution, and drying the dendrobe extracting solution in vacuum for later use; in the second step, 5g of the treated active carbon and 100ml of 0.05mol/L FeSO are taken4·7H2O solution is reacted by adopting a liquid phase reduction method until no bubbles are generated; thirdly, centrifugally separating reaction products at the speed of 4000rpm, ultrasonically cleaning for 3 times at the temperature of 35 ℃, and drying in vacuum to obtain the loaded activated carbon nano zero-valent iron; wherein the preparation of the dendrobium extract comprises the following steps: cutting stem of herba Dendrobii into segments with length of 1cm, adding 6 times of stem weight of herba Dendrobii into stem, extracting in water bath for 3 hr, and vacuum concentrating to obtain extractive solution;
step 2, when C in the saturated fatty acid is 14, namely the saturated fatty acid is tetradecanoic acid, dissolving the tetradecanoic acid in a methanol water solution, adding sodium hydroxide into the solution to wash out a precipitate, filtering, and adding the precipitate into a silver nitrate solution to obtain silver tetradecanoate; weighing silver myristate, adding hexadecyl tertiary amine, electromagnetically stirring for 2h at 60 ℃, adding cerium acetate, continuously stirring uniformly, separating out a precipitate, performing suction filtration, and performing vacuum drying to obtain modified cerium acetate, wherein the molar ratio of cerium acetate to nano-silver is 1: 0.05;
weighing 25 parts of loaded active carbon nano zero-valent iron, 8 parts of modified cerium acetate, 12 parts of potassium nitrate, 2 parts of sodium citrate, 8 parts of calcium stearate, 12 parts of sodium nitrate, 2 parts of potassium nitrate, 0.1 part of dispersant and 1 part of lubricant by weight, mixing, grinding in a ball mill, transferring into a muffle furnace, calcining for 1 hour at the speed of 5 ℃/min, and naturally cooling to obtain a semi-finished product;
and 4, washing the semi-finished product with ethanol and deionized water in sequence, circularly washing for 3 times, and drying in an oven environment at the temperature of 80 ℃ to obtain the composite antibacterial agent.
The composite antibacterial agent is applied to the preparation of synthetic resin, and the mass fraction of the antibacterial agent is 0.01%.
Example 2
A preparation method of a rare earth composite antibacterial agent doped with nano silver comprises the following steps:
step 1, firstly preparing the loaded active carbon nano zero-valent iron
Firstly, cleaning activated carbon, soaking the cleaned activated carbon in a dendrobe extracting solution for 24 hours at low temperature, taking out the dendrobe extracting solution, and drying the dendrobe extracting solution in vacuum for later use; in the second step, 8g of the treated active carbon and 100ml of 0.05mol/L FeSO are taken4·7H2O solution is reacted by adopting a liquid phase reduction method until no bubbles are generated; thirdly, centrifugally separating reaction products at the speed of 4000rpm, ultrasonically cleaning for 4 times at the temperature of 35 ℃, and drying in vacuum to obtain the loaded activated carbon nano zero-valent iron; wherein the preparation of the dendrobium extract comprises the following steps: cutting stem of herba Dendrobii into segments with length of 1-2cm, adding 7 times of stem weight of herba Dendrobii into stem, extracting in water bath for 4 hr, and vacuum concentrating to obtain extractive solution;
step 2, when C in the saturated fatty acid is 14, namely the saturated fatty acid is tetradecanoic acid, dissolving the tetradecanoic acid in a methanol water solution, adding sodium hydroxide into the solution to wash out a precipitate, filtering, and adding the precipitate into a silver nitrate solution to obtain silver tetradecanoate; weighing silver myristate, adding hexadecyl tertiary amine, electromagnetically stirring for 2h at 65 ℃, adding lanthanum acetate, continuously stirring uniformly, separating out a precipitate, performing suction filtration, and performing vacuum drying to obtain modified lanthanum acetate, wherein the molar ratio of the soluble rare earth salt to the nano silver is 1: 0.1;
weighing 30 parts of loaded active carbon nano zero-valent iron, 12 parts of modified lanthanum acetate, 14 parts of potassium nitrate, 5 parts of sodium citrate, 10 parts of calcium stearate, 15 parts of sodium nitrate, 6 parts of potassium nitrate, 0.4 part of dispersant and 1 part of lubricant by weight, mixing, grinding in a ball mill, calcining in a muffle furnace at the speed of 8 ℃/min for 2 hours, and naturally cooling to obtain a semi-finished product;
and 4, washing the semi-finished product with ethanol and deionized water in sequence, circularly washing for 4 times, and drying in an oven environment at the temperature of 80 ℃ to obtain the composite antibacterial agent.
The composite antibacterial agent is applied to the preparation of synthetic resin, and the mass fraction of the antibacterial agent is 0.04%.
Example 3
A preparation method of a rare earth composite antibacterial agent doped with nano silver comprises the following steps:
step 1, firstly preparing the loaded active carbon nano zero-valent iron
Firstly, cleaning activated carbon, soaking the cleaned activated carbon in a dendrobe extracting solution for 24 hours at low temperature, taking out the dendrobe extracting solution, and drying the dendrobe extracting solution in vacuum for later use; secondly, taking 10g of treated active carbon and 100ml of 0.05mol/L FeSO4·7H2O solution is reacted by adopting a liquid phase reduction method until no bubbles are generated; thirdly, centrifugally separating reaction products at the speed of 6000rpm, ultrasonically cleaning for 5 times at the temperature of 35 ℃, and drying in vacuum to obtain the loaded activated carbon nano zero-valent iron; the preparation method of the dendrobium extract comprises the following steps: cutting stem of herba Dendrobii into segments with length of 2cm, adding 8 times of stem weight of herba Dendrobii into stem, extracting in water bath for 4 hr, and vacuum concentrating to obtain extractive solution;
step 2, when C in the saturated fatty acid is 14, namely the saturated fatty acid is tetradecanoic acid, dissolving the tetradecanoic acid in a methanol water solution, adding sodium hydroxide into the solution to wash out a precipitate, filtering, and adding the precipitate into a silver nitrate solution to obtain silver tetradecanoate; weighing silver myristate, adding hexadecyl tertiary amine, electromagnetically stirring for 2h at 70 ℃, adding lanthanum nitrate, continuously stirring uniformly, separating out a precipitate, performing suction filtration, and performing vacuum drying to obtain modified lanthanum nitrate, wherein the molar ratio of lanthanum nitrate to nano-silver is 1: 0.1;
weighing 38 parts of loaded active carbon nano zero-valent iron, 14 parts of modified lanthanum nitrate, 18 parts of potassium nitrate, 8 parts of sodium citrate, 14 parts of calcium stearate, 18 parts of sodium nitrate, 9 parts of potassium nitrate, 0.6 part of dispersant and 5 parts of lubricant by weight, mixing, grinding in a ball mill, transferring into a muffle furnace, calcining for 3 hours, and naturally cooling to obtain a semi-finished product; wherein the heating rate is 10 ℃/min;
and 4, washing the semi-finished product with ethanol and deionized water in sequence, circularly washing for 5 times, and drying in an oven environment at the temperature of 80 ℃ to obtain the composite antibacterial agent.
The composite antibacterial agent is applied to the preparation of synthetic resin, and the mass fraction of the antibacterial agent is 0.5%.
Comparative example 1
The rest of the process is the same as the process of example 2 except that the zero-valent iron powder is used to replace the loaded active carbon nanometer zero-valent iron.
Comparative example 2
The same as in example 2 was repeated except that the modified rare earth salt was replaced with a soluble rare earth salt.
Comparative example 3
The rest of the process is the same as example 2 except that chitosan is used to replace the dendrobium extract.
Comparative example 4
The rest of the process is the same as example 2 except that the zero-valent iron powder is used to replace the loaded activated carbon nano zero-valent iron, the rare earth salt and the nano silver particles are used to replace the modified rare earth salt.
Sterilizing all the tools with an ultraviolet lamp for 30min, sucking 100 mu L of escherichia coli bacterial liquid, injecting the escherichia coli bacterial liquid into the center of a culture medium, igniting and cooling a triangular glass rod on an alcohol lamp, spreading the bacterial liquid until the surface of the whole culture medium is uniformly coated, then placing the culture medium on an antibacterial plastic sheet, placing all the culture dishes in a constant temperature box at 37 ℃ for culturing for 24h, taking out the culture dishes, observing the bacterial growth condition, and measuring the sheet and the diameter of an antibacterial spot. The diameter of the bacteriostatic circle generated by each sheet is measured, the bacteriostatic effect of the sheet can be seen by calculating the area, the larger the area is, the more obvious the bacteriostatic effect is, and the smaller the area is, the worse the bacteriostatic effect is. According to the method, the bacterial liquid is replaced by staphylococcus aureus and fungi for testing, and the test results are shown in the following table.
As can be seen from the above table, after the zero-valent iron powder, the soluble rare earth salt and the nano-silver are specially treated, the antibacterial spectrum of the obtained antibacterial agent is light, and the antibacterial effect is obvious. The antibacterial aging is carried out on the examples and the comparative examples, namely after 12 hours, the antibacterial duration of the examples 1-3 is increased by 3.0 times compared with the antibacterial duration of the comparative example 4 by taking escherichia coli as an example, and the composite antibacterial agent prepared by the method provided by the invention is further proved to have lasting antibacterial effect and high stability.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, and any simple modifications or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are within the scope of the present invention.
Claims (9)
1. A preparation method of a rare earth composite antibacterial agent doped with nano silver is characterized by comprising the following steps:
step 1, firstly preparing the loaded active carbon nano zero-valent iron
Firstly, cleaning activated carbon, soaking the cleaned activated carbon in a dendrobe extracting solution for 24 hours at low temperature, taking out the dendrobe extracting solution, and drying the dendrobe extracting solution in vacuum for later use; secondly, taking 5-10g of treated active carbon and 100ml of 0.05mol/L FeSO4·7H2The O solution is reacted by adopting a liquid phase reduction method until no bubbles are generated, and the reaction is finished; thirdly, centrifugal separation reactionUltrasonically cleaning the product at 35 ℃ for 3-5 times, and drying in vacuum to obtain the loaded activated carbon nano zero-valent iron;
step 2, dissolving saturated fatty acid in a methanol water solution, adding sodium hydroxide into the solution to wash out a precipitate, filtering, and adding the precipitate into a silver nitrate solution to obtain saturated fatty acid silver; weighing saturated fatty acid silver, adding hexadecyl tertiary amine, electromagnetically stirring for 2 hours at the temperature of 60-70 ℃, then adding soluble rare earth salt, continuously stirring uniformly, precipitating, filtering, and drying in vacuum to obtain the modified rare earth salt, wherein the molar ratio of the soluble rare earth salt to the nano-silver is 1: 0.05-0.1;
weighing 25-38 parts of loaded activated carbon nano zero-valent iron, 8-14 parts of modified rare earth salt, 12-18 parts of potassium nitrate, 2-8 parts of sodium citrate, 8-14 parts of calcium stearate, 12-18 parts of sodium nitrate, 2-9 parts of potassium nitrate, 0.1-0.6 part of dispersant and 1-5 parts of lubricant by weight, mixing, grinding in a ball mill, transferring into a muffle furnace, calcining for 1-3 hours, and naturally cooling to obtain a semi-finished product;
and 4, repeatedly washing the semi-finished product, and drying in an oven to obtain the composite antibacterial agent.
2. The method for preparing the nano-silver doped rare earth composite antibacterial agent according to claim 1, wherein the preparation of the dendrobe extracting solution in step 1 comprises the following steps: cutting stem of herba Dendrobii into segments with length of 1-2cm, adding 6-8 times of stem weight of herba Dendrobii into stem, extracting in water bath for 3-4 hr, and vacuum concentrating to obtain extractive solution.
3. The method for preparing the nano-silver doped rare earth composite antibacterial agent as claimed in claim 1, wherein the eccentricity in step 1 is 4000-6000 rpm.
4. The method for preparing a nano-silver doped rare earth composite antibacterial agent according to claim 1, wherein the soluble rare earth salt in the step 2 is cerium acetate, europium nitrate, lanthanum acetate or neodymium nitrate; the number of C in the saturated fatty acid is 10-14.
5. The method for preparing the nano-silver doped rare earth composite antibacterial agent according to claim 1, wherein the components weighed in the step 3 are as follows: 30 parts of loaded activated carbon nano zero-valent iron, 12 parts of modified rare earth salt, 14 parts of potassium nitrate, 5 parts of sodium citrate, 10 parts of calcium stearate, 15 parts of sodium nitrate, 6 parts of potassium nitrate, 0.4 part of dispersant and 1 part of lubricant.
6. The method for preparing a nano-silver doped rare earth composite antibacterial agent according to claim 1, wherein the temperature rise rate of the calcination in the step 3 is 5 to 10 ℃/min.
7. The method for preparing a nano-silver doped rare earth composite antibacterial agent according to claim 1, wherein the washing and drying steps of step 4 are as follows: washing with ethanol and deionized water sequentially, circularly washing for 3-5 times, and drying in oven at 80 deg.C.
8. A bacteriostatic synthetic resin comprising the nano-silver doped rare earth complex antibacterial agent according to any one of claims 1 to 7.
9. The bacteriostatic synthetic resin according to claim 8, wherein the bacteriostatic agent accounts for 0.01-0.5% of the bacteriostatic synthetic resin.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113967251A (en) * | 2021-10-09 | 2022-01-25 | 山东凯普润消毒灭菌技术有限公司 | Bacteriostatic agent, hand sanitizer containing bacteriostatic agent and preparation method of hand sanitizer |
| CN115582096A (en) * | 2022-10-11 | 2023-01-10 | 福建师范大学 | Carbon-doped nano zero-valent iron composite material and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531085A (en) * | 2010-12-10 | 2012-07-04 | 北京师范大学 | Method for treating oxytetracycline waste water with iron-modified attapulgite adsorbent |
| CN103566901A (en) * | 2013-09-26 | 2014-02-12 | 蚌埠华纺滤材有限公司 | Pine nut shell gas-phase adsorption active carbon and preparation method thereof |
| CN104073911A (en) * | 2014-07-17 | 2014-10-01 | 东华大学 | Preparation method for nano silver antibacterial polyester |
| CN106633310A (en) * | 2016-12-29 | 2017-05-10 | 青岛海之星生物科技有限公司 | Antibacterial and mould-proof polyethylene compound plastic masterbatch |
| CN110559990A (en) * | 2019-09-02 | 2019-12-13 | 科炭(厦门)新材料有限公司 | Preparation method of pure water carbon composite material with low nano zero-valent iron and nano silver loading |
-
2020
- 2020-07-09 CN CN202010655775.8A patent/CN111690175A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531085A (en) * | 2010-12-10 | 2012-07-04 | 北京师范大学 | Method for treating oxytetracycline waste water with iron-modified attapulgite adsorbent |
| CN103566901A (en) * | 2013-09-26 | 2014-02-12 | 蚌埠华纺滤材有限公司 | Pine nut shell gas-phase adsorption active carbon and preparation method thereof |
| CN104073911A (en) * | 2014-07-17 | 2014-10-01 | 东华大学 | Preparation method for nano silver antibacterial polyester |
| CN106633310A (en) * | 2016-12-29 | 2017-05-10 | 青岛海之星生物科技有限公司 | Antibacterial and mould-proof polyethylene compound plastic masterbatch |
| CN110559990A (en) * | 2019-09-02 | 2019-12-13 | 科炭(厦门)新材料有限公司 | Preparation method of pure water carbon composite material with low nano zero-valent iron and nano silver loading |
Non-Patent Citations (1)
| Title |
|---|
| 赵菊润 等编著: "《龙陵紫皮石斛》", 31 December 2016, 四川科学技术出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113967251A (en) * | 2021-10-09 | 2022-01-25 | 山东凯普润消毒灭菌技术有限公司 | Bacteriostatic agent, hand sanitizer containing bacteriostatic agent and preparation method of hand sanitizer |
| CN115582096A (en) * | 2022-10-11 | 2023-01-10 | 福建师范大学 | Carbon-doped nano zero-valent iron composite material and preparation method and application thereof |
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Application publication date: 20200922 |